Direct synthesis and mass spectroscopic observation of the {M40} polyoxothiometalate wheel

Miras, H.N. , Zang, H.Y., Long, D.L. and Cronin, L. (2011) Direct synthesis and mass spectroscopic observation of the {M40} polyoxothiometalate wheel. European Journal of Inorganic Chemistry, 2011(33), pp. 5105-5111. (doi: 10.1002/ejic.201100833)

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The nanosized, 2.2 nm, {Mo40} oxo(thio)metalate wheel was isolated in high yield using a direct synthetic procedure which involves acidification of a molybdate solution in the presence of the {Mo2O2S2}2+oxothio cation as the starting material. The [(Mo8O28)4(Mo2O2S2)4]24 wheel, 1a, was characterised by single-crystal X-ray diffraction analysis, IR, Raman, UV/Vis and flame atomic absorption spectroscopy (FAAS). Solid state and solution Raman spectroscopic studies allowed the unambiguous determination of the critical conditions by which compound 1 retains its integrity in solution. Electrospray ionisation mass spectrometry (ESI-MS) studies carried out on aqueous solutions of the crystalline material showed that the nanosized wheel retains its integrity in concentrated solutions. High resolution ESI-MS studies allowed the direct observation of the discrete wheel as well as the distinct self-assembly stages of its formation; from the fundamental building units through to the final formation of well resolved aggregations of 1D chains which is in agreement with the solid state studies.

Item Type:Articles
Glasgow Author(s) Enlighten ID:Moiras, Dr Haralampos and Long, Dr Deliang and Cronin, Professor Lee
Authors: Miras, H.N., Zang, H.Y., Long, D.L., and Cronin, L.
College/School:College of Science and Engineering > School of Chemistry
Journal Name:European Journal of Inorganic Chemistry
Journal Abbr.:Euro. J. Inorg. Chem
ISSN (Online):1099-0682
Published Online:18 October 2011

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